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CN102220579B - Brush-coat type phosphating solution containing rust and preparation method thereof - Google Patents

Brush-coat type phosphating solution containing rust and preparation method thereof Download PDF

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CN102220579B
CN102220579B CN201110147617.2A CN201110147617A CN102220579B CN 102220579 B CN102220579 B CN 102220579B CN 201110147617 A CN201110147617 A CN 201110147617A CN 102220579 B CN102220579 B CN 102220579B
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CN102220579A (en
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王周成
赵梓岑
严维力
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Xiamen University
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Abstract

一种涂刷型带锈磷化液及其制备方法,涉及一种磷化液。提供一种不仅具有清洁无污染、成膜快速、结合力强、耐蚀性好、操作简便、投资少、成本低等优点,而且适用于大型工件或户外设备,除油、除锈、磷化、钝化一步完成的涂刷型带锈磷化液及其制备方法。涂刷型带锈磷化液由以下原料组成磷酸、氧化锌、乙二胺四乙酸、乙醇、钼酸钠、氟化钠、硫酸镍、聚乙二醇6000、余量为水。将氧化锌加入少量水中,调成糊状;再加入磷酸,溶解后加入乙二胺四乙酸,再依次加入乙醇、钼酸钠、硫酸镍(或乙酸镍)和聚乙二醇6000,搅拌均匀后加入足量水即得所述涂刷型带锈磷化液。A brushing type rusty phosphating solution and a preparation method thereof relate to a phosphating solution. Provide a clean and pollution-free, fast film-forming, strong binding force, good corrosion resistance, easy operation, low investment, low cost, etc., and is suitable for large workpieces or outdoor equipment, oil removal, rust removal, phosphating 1. Brushing type rusty phosphating solution with passivation completed in one step and preparation method thereof. Brushing type rusty phosphating solution is composed of the following raw materials: phosphoric acid, zinc oxide, ethylenediaminetetraacetic acid, ethanol, sodium molybdate, sodium fluoride, nickel sulfate, polyethylene glycol 6000, and the balance is water. Add zinc oxide into a small amount of water to make a paste; then add phosphoric acid, dissolve and add ethylenediaminetetraacetic acid, then add ethanol, sodium molybdate, nickel sulfate (or nickel acetate) and polyethylene glycol 6000 in sequence, and stir well Then add enough water to get the brushing type rusty phosphating solution.

Description

一种涂刷型带锈磷化液及其制备方法A kind of brushing type rusty phosphating solution and preparation method thereof

技术领域 technical field

本发明涉及一种磷化液,尤其是涉及一种涂刷型带锈磷化液及其制备方法。The invention relates to a phosphating solution, in particular to a brushing type rusty phosphating solution and a preparation method thereof.

背景技术 Background technique

为了提高钢铁件表面防锈能力,通常对其表面进行磷化处理。磷化膜主要用做涂料涂装的底层,金属冷加工的润滑层,以及金属表面保护层等,可以起到防锈、减磨耐磨、润滑、增进涂料与金属基底附着力等多种作用。In order to improve the anti-rust ability of the surface of steel parts, the surface is usually phosphating. Phosphating film is mainly used as the bottom layer of paint coating, the lubricating layer of metal cold processing, and the protective layer of metal surface, etc., which can play various functions such as rust prevention, wear reduction, lubrication, and improvement of adhesion between paint and metal substrate.

对钢铁件的磷化工艺多为中高温磷化,处理前需经过除油除锈预处理,且温度高,能耗高,磷化时间长,工序繁杂。另外磷化最常采用的都是喷淋或浸泡等方式,随着磷化应用领域的扩大,这些方式已经不能适应新的情况。例如建筑、电力、海洋石油开采、冶金及采掘等领域一些钢制设备的磷化,因其体积和重量庞大,结构复杂,就不适合喷淋或浸泡。而目前磷化技术的发展方向,主要是提高质量和降低污染、节能、无毒、环保,进一步是清洁磷化,磷化液应该具有节约材料与能源、功能合理,产品在使用过程中及使用后不危害人体健康和破坏生态环境的特点。因此,一种常温快速多功能磷化工艺亟带解决,“常温快速磷化”能弥补中高温磷化的缺点,温度低、能耗小、沉渣少、晶粒细、膜薄、漆膜的附着力和耐蚀性可以大大提高;“多功能”则表示具有除油、除锈、磷化、钝化一步完成的特点,可大大节省工序,简化操作;另外,涂刷操作不需酸液槽,可大大增加该工艺的应用领域,特别适用于大型工件或室外设备的磷化处理。The phosphating process for iron and steel parts is mostly medium-high temperature phosphating, which requires degreasing and rust pretreatment before treatment, and the temperature is high, energy consumption is high, phosphating time is long, and the process is complicated. In addition, the most commonly used methods of phosphating are spraying or soaking. With the expansion of the application field of phosphating, these methods can no longer adapt to the new situation. For example, the phosphating of some steel equipment in the fields of construction, electric power, offshore oil exploitation, metallurgy and mining is not suitable for spraying or immersion because of its large volume, weight and complex structure. At present, the development direction of phosphating technology is mainly to improve quality and reduce pollution, energy saving, non-toxic, and environmental protection, and further clean phosphating. Phosphating solution should save materials and energy, and have reasonable functions. It will not endanger human health and destroy the ecological environment. Therefore, a rapid and multifunctional phosphating process at room temperature needs to be solved urgently. Adhesion and corrosion resistance can be greatly improved; "multifunctional" means that it has the characteristics of one-step completion of oil removal, rust removal, phosphating, and passivation, which can greatly save procedures and simplify operations; in addition, the brushing operation does not require acid The tank can greatly increase the application field of the process, especially suitable for phosphating treatment of large workpieces or outdoor equipment.

发明内容 Contents of the invention

本发明的目的在于提供一种不仅具有清洁无污染、成膜快速、结合力强、耐蚀性好、操作简便、投资少、成本低等优点,而且适用于大型工件或户外设备,除油、除锈、磷化、钝化一步完成的涂刷型带锈磷化液及其制备方法。The purpose of the present invention is to provide a method that not only has the advantages of clean and pollution-free, fast film formation, strong binding force, good corrosion resistance, easy operation, less investment, and low cost, but also is suitable for large workpieces or outdoor equipment, degreasing, The invention relates to a brushing type rusty phosphating solution which can complete rust removal, phosphating and passivation in one step and a preparation method thereof.

所述涂刷型带锈磷化液由以下原料组成:The brushing type rusty phosphating solution is composed of the following raw materials:

磷酸                          1392~208.8mL/L;Phosphoric acid 1392~208.8mL/L;

氧化锌                        1~3g/L;Zinc oxide 1~3g/L;

乙二胺四乙酸(EDTA)                4~10g/L;Ethylenediaminetetraacetic acid (EDTA) 4~10g/L;

乙醇                              126.6mL/L;Ethanol 126.6mL/L;

钼酸钠                            1.5~4g/L;Sodium molybdate 1.5~4g/L;

氟化钠                            1~3g/L;Sodium fluoride 1~3g/L;

硫酸镍(或乙酸镍)                  1~2g/L;Nickel sulfate (or nickel acetate) 1~2g/L;

聚乙二醇6000                      2~5g/L;Polyethylene glycol 6000 2~5g/L;

余量为水。The balance is water.

所述涂刷型带锈磷化液的制备方法包括以下步骤:The preparation method of described brushing type rusty phosphating solution comprises the following steps:

1)将氧化锌加入少量水中,调成糊状;1) Add zinc oxide into a small amount of water to make a paste;

2)再加入磷酸,溶解后加入乙二胺四乙酸,再依次加入乙醇、钼酸钠、硫酸镍(或乙酸镍)和聚乙二醇6000,搅拌均匀后加入足量水即得所述涂刷型带锈磷化液。2) Add phosphoric acid, add ethylenediaminetetraacetic acid after dissolving, then add ethanol, sodium molybdate, nickel sulfate (or nickel acetate) and polyethylene glycol 6000 in sequence, stir evenly, add sufficient water to obtain the coating Brush type rust phosphating solution.

所述涂刷型带锈磷化液的使用方法为:The using method of the brushing type rusty phosphating solution is:

1)钢铁件预处理1) Pretreatment of steel parts

普通带锈钢铁件不需前期预处理,锈量大的钢铁件可使用砂纸或钢铲除掉过多的锈壳和浮灰即可。Ordinary rusted steel parts do not require pre-treatment. For steel parts with a large amount of rust, sandpaper or steel can be used to remove excessive rust shells and floating ash.

2)钢铁件的磷化处理2) Phosphating treatment of steel parts

使用耐酸刷直接将磷化液在铁件上均匀的涂刷一层液膜,然后等待其自然干燥后即可。Use an acid-resistant brush to directly apply a layer of phosphating solution evenly on the iron piece, and then wait for it to dry naturally.

本发明所述涂刷型带锈磷化液使用后所形成的磷化膜黑亮致密,厚度可达100μm,结合力佳,CuSO4点滴实验,按GB/T 6807-1986中规定进行检测,液滴变为淡红色所需时间可达到470s;中型盐雾实验,按GB/T 10125-1997中规定进行检测,12h以上无锈痕。The phosphating film formed by the brushing type rusty phosphating solution of the present invention is black, bright and compact, with a thickness of up to 100 μm and good binding force. The CuSO 4 drip test is tested according to the regulations in GB/T 6807-1986. The time required for the droplet to turn into light red can reach 470s; the medium-sized salt spray test shall be tested according to the provisions of GB/T 10125-1997, and there will be no rust marks for more than 12 hours.

实验证明,经过本发明所述涂刷型带锈磷化液处理后的所形成的磷化膜显示出表面含裂纹的膜结构,这种结构在其作为涂料涂装底层时显示出其独特的优越性,通过涂料向裂纹的渗透,涂料和磷化膜间的咬合作用,使其漆膜附着力得到有效的提高。按GB-T1720-1979中规定进行检测,漆膜附着力不小于1级。Experiment proves that the formed phosphating film after the brushing type rust phosphating solution treatment of the present invention shows the film structure containing cracks on the surface, and this structure shows its unique characteristics when it is used as the coating bottom layer. Superiority, through the penetration of the paint into the cracks, the bite between the paint and the phosphating film, the adhesion of the paint film is effectively improved. Tested according to the provisions of GB-T1720-1979, the adhesion of the paint film is not less than grade 1.

附图说明 Description of drawings

图1为经本发明实施例所述涂刷型带锈磷化液处理后磷化膜表面形貌SEM图。在图1中,标尺为20μm。Fig. 1 is an SEM image of the surface morphology of the phosphating film after being treated with the brushing type rusty phosphating solution described in the embodiment of the present invention. In Figure 1, the scale bar is 20 μm.

具体实施方式Detailed ways

实施例1Example 1

本发明所述涂刷型带锈磷化液由以下原料组成:The brushing type rusty phosphating solution of the present invention is made up of following raw material:

磷酸                    174mL/L;Phosphoric acid 174mL/L;

氧化锌                  1.6g/L;Zinc oxide 1.6g/L;

EDTA                    6g/L;EDTA 6g/L;

乙醇                    126.6mL/L;Ethanol 126.6mL/L;

钼酸钠                  1.5g/L;Sodium molybdate 1.5g/L;

氟化钠                  1g/L;Sodium fluoride 1g/L;

硫酸镍                  2g/L;Nickel sulfate 2g/L;

聚乙二醇6000            2g/L;Polyethylene glycol 6000 2g/L;

水                      余量。Water balance.

将氧化锌加入少量水中,调成糊状,然后加入磷酸,搅拌至充分溶解。加入EDTA,搅拌至充分溶解。然后依次加入乙醇,钼酸钠,硫酸镍,聚乙二醇6000,搅拌均匀,最后加入足量水即可。采用涂刷的方式处理锈迹严重的铁门,成膜效果佳,膜层呈亮黑色,漆膜结合力佳。Add zinc oxide into a small amount of water to make a paste, then add phosphoric acid and stir until fully dissolved. Add EDTA and stir until fully dissolved. Then add ethanol, sodium molybdate, nickel sulfate, polyethylene glycol 6000 in turn, stir evenly, and finally add enough water. The iron door with serious rust is treated by brushing, the film forming effect is good, the film layer is bright black, and the paint film has good adhesion.

实施例2Example 2

本发明所述涂刷型带锈磷化液由以下原料组成:The brushing type rusty phosphating solution of the present invention is made up of following raw materials:

磷酸                    208.8mL/L;Phosphoric acid 208.8mL/L;

氧化锌                  1g/L;Zinc oxide 1g/L;

EDTA                    10g/L;EDTA 10g/L;

乙醇                    126.6mL/L;Ethanol 126.6mL/L;

钼酸钠                  2.5g/L;Sodium molybdate 2.5g/L;

氟化钠                  3g/L;Sodium fluoride 3g/L;

硫酸镍                  1.5g/L;Nickel sulfate 1.5g/L;

聚乙二醇6000            4g/L;Polyethylene glycol 6000 4g/L;

水                      余量。Water balance.

磷化液配制方法同实施例1。采用涂刷的方式操作,处理锈迹严重的铁制船壳,效果佳,膜层亮黑,结合力强。The preparation method of phosphating solution is the same as in Example 1. It is operated by brushing to deal with the iron ship hull with serious rust, the effect is good, the film layer is bright black, and the bonding force is strong.

实施例3Example 3

本发明所述涂刷型带锈磷化液由以下原料组成:The brushing type rusty phosphating solution of the present invention is made up of following raw material:

磷酸                    139.2mL/L;Phosphoric acid 139.2mL/L;

氧化锌                  3g/L;Zinc oxide 3g/L;

EDTA                    4g/L;EDTA 4g/L;

乙醇                    126.6mL/L;Ethanol 126.6mL/L;

钼酸钠                  2g/L;Sodium molybdate 2g/L;

氟化钠                  1.5g/L;Sodium fluoride 1.5g/L;

乙酸镍                  2g/L;Nickel acetate 2g/L;

聚乙二醇6000            3g/L;Polyethylene glycol 6000 3g/L;

水                      余量。Water balance.

磷化液配制方法同实施例1。采用涂刷的方式操作,处理锈迹严重的铁制支架,效果佳,膜层亮黑,结合力强。The preparation method of phosphating solution is the same as in Example 1. It is operated by brushing to deal with the iron bracket with serious rust. The effect is good, the film layer is bright and black, and the bonding force is strong.

实施例4Example 4

本发明所述涂刷型带锈磷化液由以下原料组成:The brushing type rusty phosphating solution of the present invention is made up of following raw materials:

磷酸                    139.2mL/L;Phosphoric acid 139.2mL/L;

氧化锌                  2.5g/L;Zinc oxide 2.5g/L;

EDTA                    8g/L;EDTA 8g/L;

乙醇                    126.6mL/L;Ethanol 126.6mL/L;

钼酸钠                  4g/L;Sodium molybdate 4g/L;

氟化钠                  2.5g/L;Sodium fluoride 2.5g/L;

乙酸镍                  1g/L;Nickel acetate 1g/L;

聚乙二醇6000            5g/L;Polyethylene glycol 6000 5g/L;

水                      余量。Water balance.

磷化液配制方法同实施例1。采用涂刷的方式操作,处理锈迹严重的农用打谷机铁制外壳,效果佳,膜层黑亮,硬度高。The preparation method of phosphating solution is the same as in Example 1. It is operated by brushing to deal with the iron casing of the agricultural threshing machine with serious rust. The effect is good, the film layer is black and bright, and the hardness is high.

由图1可见,经过本发明所述涂刷型带锈磷化液处理后的所形成的磷化膜显示出表面含裂纹的膜结构,这种结构在其作为涂料涂装底层时显示出其独特的优越性,通过涂料向裂纹的渗透,涂料和磷化膜间的咬合作用,使其漆膜附着力得到有效的提高。按GB-T1720-1979中规定进行检测,漆膜附着力不小于1级。As can be seen from Fig. 1, the formed phosphating film after the brushing type rust phosphating solution treatment of the present invention shows the film structure containing cracks on the surface, and this structure shows its properties when it is used as the coating bottom layer. Unique superiority, through the penetration of the paint into the cracks, the bite between the paint and the phosphating film, the adhesion of the paint film is effectively improved. Tested according to the provisions of GB-T1720-1979, the adhesion of the paint film is not less than grade 1.

Claims (2)

1. a brush-coat type phosphating solution containing rust, is characterized in that its raw material consists of:
2. the preparation method of a kind of brush-coat type phosphating solution containing rust as claimed in claim 1, is characterized in that comprising the following steps:
1) zinc oxide is added in a small amount of water, furnishing pasty state;
2) add phosphoric acid again, after dissolving, add ethylenediamine tetraacetic acid (EDTA), then add ethanol successively, Sodium orthomolybdate, single nickel salt or nickelous acetate, polyethylene glycol 6000, add enough water after stirring and namely obtain described brush-coat type phosphating solution containing rust.
CN201110147617.2A 2011-06-02 2011-06-02 Brush-coat type phosphating solution containing rust and preparation method thereof Active CN102220579B (en)

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Publication number Priority date Publication date Assignee Title
CN102644072B (en) * 2012-04-01 2014-04-09 清华大学 Composition for phosphating steel and iron and application thereof
CN102605363B (en) * 2012-04-17 2013-11-20 安徽启明表面技术有限公司 Room-temperature type quick-drying brushing type phosphorizing liquid and preparation method thereof
CN102691058A (en) * 2012-06-19 2012-09-26 厦门市冠达鑫环保科技有限公司 Phosphorizing liquid and production method thereof

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CN1066894A (en) * 1992-04-21 1992-12-09 陈金田 The low temperature fast phosphating agent

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
CN1066894A (en) * 1992-04-21 1992-12-09 陈金田 The low temperature fast phosphating agent

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